CN216499293U

CN216499293U - Gradient cooling device in chiral salifying splitting process

Info

Publication number: CN216499293U
Application number: CN202122401162.4U
Authority: CN
Inventors: 马飞鸿; 杜项龙; 马士忠
Original assignee: Shanghai Hanhong Technology Co ltd
Current assignee: Shanghai Hanhong Technology Co ltd
Priority date: 2021-10-03
Filing date: 2021-10-03
Publication date: 2022-05-13
Anticipated expiration: 2031-10-03

Abstract

The utility model discloses a gradient cooling device in a chiral salifying and splitting process, and belongs to the technical field of fine chemical engineering. Gradient heat sink in chirality salification split process, including the supporting seat, still include: the temperature control box is fixedly connected to the supporting seat through a supporting rod; the reaction kettle is fixedly connected in the temperature control box through a support frame; the refrigerating assembly is fixedly connected to the supporting seat; the temperature conducting pipe is arranged in the temperature control box; the vacuum pump is fixedly connected to the supporting seat, wherein the output end of the vacuum pump is communicated with the temperature control box through an air guide pipe, the air guide pipe is communicated with a pressure relief pipe, and an adjustable pressure valve is arranged on the pressure relief pipe; the utility model can increase the pressure in the temperature control box through the vacuum pump to improve the freezing point of purified water in the temperature control box to reduce the temperature of the ice-water mixture, thereby continuously cooling the diastereoisomers in the solution at a constant temperature, improving the purity of the isomers resolved in the chiral salt-forming resolution process and improving the chiral salt-forming resolution efficiency.

Description

Gradient cooling device in chiral salifying splitting process

Technical Field

The utility model relates to the technical field of fine chemical engineering, in particular to a gradient cooling device in a chiral salifying and splitting process.

Background

The chiral salt-forming resolution is implemented by converting two enantiomers in a racemate into diastereoisomers by a chemical reaction method through a chiral reagent, then separating the diastereoisomers through a physical or chemical method by utilizing the difference of material properties and chemical properties among the diastereoisomers, and regenerating and reducing the separated diastereoisomers into the original enantiomers through a chemical reaction. The key point of the resolution is that a proper chiral resolving agent and organic solvent combination is optimally selected.

Diastereoisomers are resolved by methods with different physical properties (mainly solubility difference in the same organic solvent), a plurality of diastereoisomers are resolved by crystallization in different solvents, and a cooling device used in the existing chiral salt-forming resolution process is difficult to control the gradient of cooling, so that the purity of the diastereoisomers obtained by cooling resolution is not high, and the requirement of chiral salt-forming resolution cannot be met.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the problem that the cooling gradient of a cooling device is difficult to control in chiral salt-forming resolution in the prior art.

In order to achieve the purpose, the utility model adopts the following technical scheme:

gradient heat sink in chirality salify split process, including the supporting seat, still include: the temperature control box is fixedly connected to the supporting seat through a supporting rod; the reaction kettle is fixedly connected in the temperature control box through a support frame; the refrigerating assembly is fixedly connected to the supporting seat; the temperature guide pipe is arranged in the temperature control box, the temperature guide pipe is spirally sleeved outside the reaction kettle, and two ends of the temperature guide pipe extend to the outside of the reaction kettle and are respectively communicated with the output end and the input end of the refrigeration assembly; the vacuum pump is fixedly connected to the supporting seat and communicated with the temperature control box through an air guide pipe, wherein the output end of the vacuum pump is communicated with the temperature control box through the air guide pipe, the air guide pipe is communicated with a pressure relief pipe, and the pressure relief pipe is provided with an adjustable pressure valve.

In order to accelerate the speed of chirality salification split, preferably, fixedly connected with motor on the reation kettle, motor output fixedly connected with pivot, pivot one end extends to a plurality of puddlers of fixedly connected with in the reation kettle.

In order to check the air pressure in the temperature control box in real time, a pressure gauge is preferably arranged on the air guide pipe.

In order to check the temperature in the temperature control box in real time, a thermometer is fixedly connected to the temperature control box and used for measuring the temperature in the temperature control box.

In order to conveniently pour the solution dissolved with the diastereoisomer into the reaction kettle, preferably, the top of the reaction kettle is communicated with a feeding pipe, the bottom of the reaction kettle is communicated with a discharging pipe, one end of the discharging pipe, far away from the reaction kettle, extends out of the temperature control box, and the reaction kettle is embedded with an observation window.

In order to facilitate pouring of purified water into the temperature control box, the top of the temperature control box is communicated with a water inlet pipe, and the bottom of the temperature control box is communicated with a water drain pipe.

Compared with the prior art, the utility model provides a gradient cooling device in the chiral salifying and splitting process, which has the following beneficial effects:

1. this gradient heat sink in chirality salification split process pressurizes in the temperature control box through the vacuum pump to reduce the freezing point of the interior pure water of temperature control box, thereby reduce the ice water mixture temperature that generates in the temperature control box, be used for cooling to the reation kettle inner solution.

2. According to the gradient cooling device in the chiral salt-forming splitting process, purified water in the temperature control box is cooled through the refrigeration assembly, the purified water is frozen to generate an ice-water mixture, in the process of absorbing heat in the reaction kettle, part of ice can be melted to absorb heat, and the temperature of the ice-water mixture is kept at a constant temperature all the time.

3. This gradient heat sink in chirality salification split process, through adjusting the adjustable pressure valve of locating on the pressure release pipe, come to adjust the atmospheric pressure in the temperature control box to make the frozen water mixture in the temperature control box carry out rapid temperature variation, thereby reach the purpose of gradient cooling, improve the efficiency that improves chirality salification split.

The parts which are not involved in the device are the same as or can be realized by the prior art, the temperature of the ice-water mixture can be reduced by increasing the pressure in the temperature control box through the vacuum pump so as to improve the freezing point of purified water in the temperature control box, so that the diastereoisomer in the solution is continuously cooled at the temperature, the purity of the isomer obtained by resolution in the chiral salt-forming resolution process is improved, and the chiral salt-forming resolution efficiency is improved.

Drawings

FIG. 1 is a first front view of a gradient cooling device in a chiral salt formation resolution process according to the present invention;

fig. 2 is a second front view of the gradient cooling device in the chiral salt formation resolution process provided by the present invention.

In the figure: 1. a supporting seat; 2. a temperature control box; 201. a thermometer; 202. a drain pipe; 203. a water inlet pipe; 3. a reaction kettle; 301. a feed tube; 302. a discharge pipe; 303. an observation window; 4. a refrigeration assembly; 401. a heat conducting pipe; 5. a vacuum pump; 501. an air duct; 502. a pressure gauge; 503. a pressure relief pipe; 504. an adjustable pressure valve; 6. a motor; 601. a rotating shaft; 602. a stirring rod.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.

Example (b):

referring to fig. 1-2, gradient heat sink in chiral salifying split process, including supporting seat 1, still include: the temperature control box 2 is fixedly connected to the supporting seat 1 through a supporting rod; the reaction kettle 3 is fixedly connected in the temperature control box 2 through a support frame; the refrigerating assembly 4 is fixedly connected to the supporting seat 1; the temperature guide pipe 401 is arranged in the temperature control box 2, wherein the temperature guide pipe 401 is spirally sleeved outside the reaction kettle 3, and two ends of the temperature guide pipe 401 extend to the outside of the reaction kettle 3 and are respectively communicated with the output end and the input end of the refrigeration component 4; vacuum pump 5, fixed connection is on supporting seat 1, is linked together through air duct 501 and accuse temperature case 2, and wherein, the output of vacuum pump 5 is linked together through air duct 501 and accuse temperature case 2, and the intercommunication has pressure release pipe 503 on the air duct 501, is equipped with adjustable pressure valve 504 on the pressure release pipe 503.

Fixedly connected with motor 6 on reation kettle 3, 6 output end fixedly connected with pivot 601 of motor, pivot 601 one end extends to a plurality of puddlers 602 of fixedly connected with in reation kettle 3, be equipped with manometer 502 on the air duct 501, fixedly connected with thermometer 201 on the accuse temperature case 2, be used for measuring the temperature in the accuse temperature case 2, 3 top intercommunications of reation kettle have filling tube 301, 3 bottom intercommunications of reation kettle have row material pipe 302, it keeps away from 3 one end of reation kettle and extends to outside the accuse temperature case 2 to arrange material pipe 302, the gomphosis has observation window 303 on reation kettle 3, 2 top intercommunications of accuse temperature case have inlet

tube

203, 2 bottom intercommunications of accuse temperature case have drain pipe 202, accuse temperature case 2 is transparent heat preservation material.

In this equipment use, can let in proper amount of pure water to the accuse temperature case 2 through inlet tube 203 earlier, specific maximum can not exceed ten of eleven of accuse temperature case 2 internal volume, seal inlet tube 203, start refrigeration subassembly 4 refrigeration, specific refrigeration subassembly 4 can be by refrigeration compressor, a condenser, the compression refrigeration mechanism that choke valve and evaporimeter are constituteed, lead into the thermal conductance pipe 401 inner loop with the refrigerant liquid, the part that thermal conductance pipe 401 is located accuse temperature case 2 is the heliciform, can fully contact with the pure water in the accuse temperature case 2, can carry out the reducing temperature to the pure water through the heat transfer of refrigerant liquid and pure water, the temperature in the accuse temperature case 2 is looked over in real time to specific accessible thermometer 201.

Meanwhile, the vacuum pump 5 is started, the temperature control box 2 is filled with air through the air duct 501, the corresponding air pressure is increased according to the constant temperature required by purified water in the temperature control box 2, when the crystallization temperature of diastereoisomer required to be separated in the solution is below 0 ℃, the vacuum pump 5 can be used for filling air into the temperature control box 2, because the freezing point of the purified water in normal atmospheric pressure is 0 ℃, when the air pressure rises, the freezing point of the purified water rises, it is required to be noted that the freezing point of the purified water can be reduced when the pressure is below 2200 atmospheric pressures, when the pressure exceeds 2200 atmospheric pressures, the freezing point of the purified water rises, so that the freezing point of the purified water in the temperature control box 2 can be reduced by pressurizing the vacuum pump 5, at the moment, when the temperature of the purified water in the temperature control box 2 is reduced to the freezing point under the action of the refrigerating assembly 4, the purified water freezes and releases heat, the released heat continuously exchanges heat with the refrigerating fluid circulating in the heat conducting tube 401 for cooling until most of the purified water in the temperature control box 2 is frozen, the operation of the refrigerating assembly 4 is stopped, the frozen purified water can expand to eleven times of the volume of the water per se, so that the volume of the purified water cannot exceed ten tenths of the volume of the temperature control box 2 when being added, the purified water is prevented from freezing and expanding to damage the temperature control box 2, the purified water in the temperature control box 2 is a mixture of liquid purified water and solid ice at the same time, the temperature of the mixture is the freezing point of the purified water at this time, the diastereomer solution needing to be separated into salt is poured into the reaction kettle 3 through the feeding tube 301, the solution exchanges heat with the ice-water mixture outside the reaction kettle 3 for cooling, so that the diastereomer is crystallized and separated out, and can be observed through the observation window 303 embedded in the reaction kettle 3, the motor 6 is started, the rotating shaft 601 is driven to rotate by the motor 6, so that the stirring rod 602 is driven to rotate in the reaction kettle 3 to stir the poured solution, the solution cooling speed can be further increased, heat can be conducted into the ice-water mixture in the solution cooling process, ice in the ice-water mixture can be melted to absorb the heat at the conduction part, and therefore the temperature of the ice-water mixture is ensured to be kept unchanged all the time before the ice is not completely melted, a stable low-temperature environment is provided for the solution in the reaction kettle 3, the purity of the precipitated diastereomer in the splitting process is improved, the precipitated diastereomer is discharged through the discharge pipe 302, the volume of the ice-water mixture in the temperature control box 2 can be changed in the process that purified water is frozen into the ice-water mixture, and in order to control the pressure in the temperature control box 2 to be always stabilized at a required pressure value, a pressure relief pipe 503 is communicated with the air guide pipe 501, be equipped with adjustable pressure valve 504 on the pressure release pipe 503, adjust adjustable pressure valve 504 to fixed value, guarantee vacuum pump 5 to lasting the pressurized in-process of control temperature box 2, the internal gas pressure of air duct 501 is stable all the time for fixed atmospheric pressure, when the pure water volume changes in control temperature box 2, the atmospheric pressure in control temperature box 2 can be through the regulation fast and stable at required atmospheric pressure value of adjustable pressure valve 504, the internal gas pressure value of control temperature box 2 is looked over in real time to accessible manometer 502 in the concrete use.

When the ice-water mixture in the temperature control box 2 needs to be subjected to gradient cooling, the adjustable pressure valve 504 can be adjusted through adjustment, so that the air pressure in the air guide pipe 501 rises, the air pressure in the temperature control box 2 continues to increase, the freezing point of the purified water in the temperature control box 2 continues to decrease, part of ice blocks in the ice-water mixture in the temperature control box 2 can be rapidly melted and absorb heat, the ice-water mixture is cooled to the temperature corresponding to the air pressure at the moment, the gradient cooling of the temperature in the temperature control box 2 is realized, the solution in the reaction kettle 3 is conveniently subjected to gradient cooling, the other diastereomer is separated out, and the purified water can be discharged through the water discharge pipe 202 after chiral salt separation is completed.

When the crystallization temperature of the diastereoisomer to be resolved in the solution is above 0 ℃, other substances with higher freezing points can be poured into the water inlet pipe 203, such as glycerol, and the like, the air pressure in the temperature control box 2 is adjusted through the vacuum pump 5, the freezing point of the substances in the temperature control box 2 is reduced to the required temperature, the substances in the temperature control box 2 are cooled to the freezing point through the refrigerating assembly 4, so that the mixture state of the solid substance and the liquid is kept, the solution in the reaction kettle 3 is cooled, and the diastereoisomer is resolved.

According to the utility model, the temperature of the ice-water mixture is reduced by increasing the pressure in the temperature control box 2 through the vacuum pump 5 so as to improve the freezing point of purified water in the temperature control box 2, so that the diastereoisomers in the solution are continuously cooled at a constant temperature, the purity of the resolved isomers in the chiral salt-forming resolution process is improved, and the chiral salt-forming resolution efficiency is improved.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and equivalent alternatives or modifications according to the technical solution of the present invention and the inventive concept thereof should be covered by the scope of the present invention.

Claims

1. Gradient heat sink in chirality salify split process, including supporting seat (1), its characterized in that still includes: the temperature control box (2) is fixedly connected to the supporting seat (1) through a supporting rod; the reaction kettle (3) is fixedly connected in the temperature control box (2) through a support frame; the refrigerating assembly (4) is fixedly connected to the supporting seat (1); the temperature guide pipe (401) is arranged in the temperature control box (2), wherein the temperature guide pipe (401) is spirally sleeved outside the reaction kettle (3), and two ends of the temperature guide pipe (401) extend to the outside of the reaction kettle (3) and are respectively communicated with the output end and the input end of the refrigeration assembly (4); the vacuum pump (5) is fixedly connected to the supporting seat (1) and communicated with the temperature control box (2) through an air duct (501), wherein the output end of the vacuum pump (5) is communicated with the temperature control box (2) through the air duct (501), the air duct (501) is communicated with a pressure relief pipe (503), and the pressure relief pipe (503) is provided with an adjustable pressure valve (504).

2. The gradient cooling device in the chiral salt-forming resolution process of claim 1, wherein a motor (6) is fixedly connected to the reaction kettle (3), a rotating shaft (601) is fixedly connected to an output end of the motor (6), and one end of the rotating shaft (601) extends into the reaction kettle (3) and is fixedly connected with a plurality of stirring rods (602).

3. The gradient cooling device in the chiral salt-forming resolution process of claim 1, wherein a pressure gauge (502) is arranged on the gas-guide tube (501).

4. The gradient cooling device in the chiral salt-forming resolution process according to claim 3, wherein a thermometer (201) is fixedly connected to the temperature control box (2) and is used for measuring the temperature in the temperature control box (2).

5. The gradient cooling device in the chiral salt-forming resolution process of claim 1, wherein the top of the reaction kettle (3) is communicated with a feeding pipe (301), the bottom of the reaction kettle (3) is communicated with a discharging pipe (302), one end of the discharging pipe (302) far away from the reaction kettle (3) extends out of the temperature control box (2), and the reaction kettle (3) is embedded with an observation window (303).

6. The gradient cooling device in the chiral salt-forming resolution process according to claim 1, wherein the top of the temperature control box (2) is communicated with a water inlet pipe (203), and the bottom of the temperature control box (2) is communicated with a water outlet pipe (202).